Аннотация:The regioselective one-pot sp3 C–H bond functionalization of an alkyl unit in organic molecules already bearing functional groups is of great interest for the synthesis of bifunctional compounds. This report describes the unprecedented regioselective synthesis of otherwise inaccessible bifunctional neo-compounds via C–H activation of an alkyl chain of linear acyl halides in the presence of CO and two different sequentially introduced nucleophiles.